Method of producing non-hygroscopic albuminous preparations.



UNITED STATES PATENT OFFICE, A

' ma'z QUADE, BERLIN, GERMANY, assrenon ro THE mit or 403mm 4 wtiLEme, or BERLIN, GERMANY.

METHOD OF PRODUCING NON -HYGROSCQPIC A'LBUMINOUS PREPARATIONS.

N0 Drawin To all whom it may concern:

- Be it known that I, Fnrrz QUADE, Dogtor of Chemistry, a citizen of the Empire of Germany, residing at Berlin, in the Empire 5 of Germany, have invented a new and use,

a form easily to be dosed out fortwo causes,

viz.:.1. During the esterification by-prod nets are easily formed which hinder the crystallization. 2. The sodium' salts are most hygroscopic, crystallize very slowly,

and furnish, even if very pure solutions are employed, a pasty crystal-mass interspersed with syrupy constituents'which mass is difficult of filtration. r

It is only possible to prevent the forma-' tion of by-products, if, for example, sodiummetaphosphate in a finely divided state, is

heated in 'vacuo with an excess of glycerin while preventing the temperature from ex (ceding 145 centigra'de, whereby nearly the whole phosphate is esterified without forming pyroester and other defiling by-products by reason of the comparatively low temperature. However, it was impossible for the phosphateformed owing to its small 'crys-.

tallizing power to separate quantitatively from the reacting mixture containin an excess of lycerin obtained by the a ove method or Iny other similarmethods. Also the addition of sodium in a quantity required for converting monoglycerophos phate into diglycerophosphate, that is in the form of sodium hydroxid, did notfurnish the desired result.

I have discovered, that a quantitative separation of the formed mono-sodium-glyecerophosphate direct from the reacting mix-' ture is rendered possible by the addition of casein-sodium, at best in alcoholic suspension, to the reacting mixture, and that thus a preparation is obtained which is useful both as a food and as a tonic. In man- Specification of Letters Patent. Application filed July 7, 1910,. Serial No. 570.825.

Patented Sept, 12, 1911.

nor a product is formed, which contains the entire qllflllllty of esterified phosphate,

-while the excess in glycerin soluble n alcohol can be easily removed by filtration. The product formed does not show the pasty state of the pure glycerophosphate, even if it contain 20% and more of glycerophosphate, proves to be non-hygroscopic, can be easily dosed out, and possesses a, taste far more agreeable than the pures lt.

I am aware, that it has already been proposed to render albumin soluble by means of disodium glycerophospliate already sepa rated from the reacting mixture and freed in any known manner from the by-product's, this pure disodium glycerophosphate serving for dissolving freshly precipitated coagulated milk, (casein). it i The method according to my invention differs from the above method in that a reacting mixture containing mono-glycerophosphate obtained by esterification is'at once employed. A second difference resides in the fact-, that not freshly precipitated casein is rendered, soluble, but an already an soluble product, viz. the case n-Sodium to be had as an article of commerce, em-v ployed, which is-siinply to serve as a vehicle for the mono-sodium-glycerophosphate. In

the present case a casein-sodium containing 54 1% sodium, acting neutral upon phenolphthalein ispreferable, The proportion between the casein-sodium and the monosodium-glycerophosphate can be varied within wide limits, while invariably useful products are obtained. Non-hygroscopic products having useful properties can be produced up to a maximum ercentage of about 25% of the mono-soc iinm-glycerophosphate. The reacting mixture serving 2? as; the raw material for this method can be produced in many various manners, and the quantity'of casein-sodium to be added can be varied: I I

Following is anexample: One part by weight of sodium-metaphosphate is dissolved. in a just sufiicient quantity of water and is heated in vacuo with three parts by weight of glycerin, whereby first the water is evaporated and then the phosphate in a finely divided state is separated in he g,lyc erin. By increasing the temperature the entire phosphate will be dissolved and at a temperature of c'enti rade the esterification will be finished. he mixture now 0 serving as raw material for the new method is in its hot state mixed with a like volume of water, and the solution so obtained is allowed to cool, after which it is introby digesting with alcohol, and can then beseparated without difiiculty from the mixture, of alcohol and .glycerin by filtration, and finally drying. If use is made of casein- -sodium containing 1% of Na., the product obtained, which contains the entire quantity of the esterized phosphate, will be soluble in cold water.

I claim 1. The hereindescribed method of producing a non-hygroscopic albuminous prepara- 7 tion, which consists in mixing alkali phosphate with glycerin, heating the mixture in vacuo whereby the phosphate is separated in a divided state in the glycerin, increasing the temperature for dissolving and esterifying the phosphate, adding water to the mixture and allowing to cool, introducing the mixture into a menstruum containing casein-alkali while agitating the entire mixture, digesting the mixture, separating the product consisting of the combination of casein-alkali with alkali glycerophosphate by filtration from the mixture, and finally drying the product.

2. The hereindescribed method of producin a non h rosco ic albuminous re aration, which consists in mixing alkali phosphate, water, and glycerin, heating the mixture in vacuo whereby the water is evaporated and the phosphate is separated in a divided state in the glycerin,

further heating the mixture to a temperature of about 145 C. soas to dissolve and esterify the phosphate, addin water to the mixture and allowing to coo introducing the mixture into a menstruum containing casein-sodium while agitating the entire mixture, digesting the mixture,.

separating the product. consisting of the combination of casein-sodium with alkali.

glycerophosphate by filtration from the mixture, and finally drying the product.

3'. The hereindescribed method of producing a non-hygroscopic albuminous preparation, which consists in preparing the raw 1 material b dissolving alkali phosphate in water, adding glycerin to the solution, heating the mixture in 'vacuo for evaporating the water and separating the phosphate in a divided state in the glycerin, increasin the .temperature for dissolving and esteri ing the phosphate, then in mixing the mixture while still warm with water, allowing it to cool, introducing the mixture into an alco- -holic suspension of casein-alkali while a 'itating the entire mixture, digesting t e mixture, separating the product by filtration from the mixture of alcohol and glycerin,

and drying it.

4. The hereindescribed method of producing a non-hygroscopic albuminous preparation, which consists in preparing the raw material by dissolving alkali phosphate in water, adding glycerin to the solution, heating the mixture in 'vaono for evaporating the water and separating the phosphate in a divided state in the glycerin, increasing the temperature of the mixture to about 145 C. so as to dissolve and esterify the phosphate, adding water to the mixture and allowing to cool, introducing the mixture into a menstruum containing casein-sodium containing 1% of sodium while agitating the entire mixture, digesting the mixture, separating the product consisting of 'the combination of casein-sodium withalkali glycerophosphate by filtration from the mixture,

and finally drying the product.

5. The hereindescribed method of producing a non-hygroscopic albuminous preparation, which consists in preparing the raw material by dissolving sodium-metaphosphate in water, adding glycerin to the solution, heating the mixture in 0.10140 for evaporating the water and separating the phosphate in a divided state in the glycerin,

increasing the temperature for dissolving and esterifying the phosphate, then in mixing the mixture while still warm with water, allowing it to cool, introducing the mixture into an alcoholic suspension of caseinsodium while agitating the entire mixture, digesting the mixture, separating the product by filtration from the mixture of alcohol and glycerin, and drying it.

v 6. The hereindescribed method of producing a non-hygroscopic albuminous preparation, which consists in preparing the raw material by dissolving sodium metaphosphate in water, adding three parts of glycerin to the solution of sodium metaphosphate, heating the mixture in vacuo for evaporating the water and separating the phosphate in a divided state in the glycerin,

increasing the temperature of the mixture sodium glycerohosphate by filtration from the mixture, an finally drying the' product.

7.. The hereindescribed method of producing a non-hygroscopic albuminous preparation, which consists in preparing the raw material by dissolving sodium metaphosphate in water, adding three parts of glycerin to the solution of sodiumm'etaphosphate, heatin the mixture in vacuo for evaporating phosphate in a divided state in the glycerin, increasin the temperature of the mixture to 145 so as to dissolve and completely esterify the phosphate, mixing the material in its hot state with about an equal volume t e water and separating the of water, allowing the solution soohtained to cool, introducing the mixture into a menstruum consisting of 20 parts casein-sodium suspended in 200 parts of 90%- alcohol wh1le agitating the entire mixture, digesting the mixture for about half an hour at the temperature. of the room,"separating the product by filtration from the mixture of 1 alcohol and Witnesses: v

' Max LEMCKE,

LOUIS VANDORN. 

